CN101659402A - Method for improving quality of oxammonium hydrochloride - Google Patents
Method for improving quality of oxammonium hydrochloride Download PDFInfo
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- CN101659402A CN101659402A CN200910018411A CN200910018411A CN101659402A CN 101659402 A CN101659402 A CN 101659402A CN 200910018411 A CN200910018411 A CN 200910018411A CN 200910018411 A CN200910018411 A CN 200910018411A CN 101659402 A CN101659402 A CN 101659402A
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- oxammonium hydrochloride
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Abstract
The invention relates to a method for improving the quality of oxammonium hydrochloride, which belongs to preparation of hydroxylamine compounds, in particular to a method for improving the quality ofproducts in the process of preparing the oxammonium hydrochloride. The method is characterized in that: in the conventional oxammonium hydrochloride production technology process, at least one filtering device is added, so that oxammonium hydrochloride solution generated by acidifying and hydrolyzing nitromethane through hydrochloric acid is filtered by the filtering device and then enters a condensation working section. The invention provides a method, which has less investment and simple operation process, eliminates black spots in the products, ensures that products cannot turn yellow in the storage life and obviously improves the quality of the oxammonium hydrochloride. The products have no black spots and impurities and cannot change color after being stored for two years. The invention not only suitable for process improvement on preparing the oxammonium hydrochloride by acidifying and hydrolyzing the nitromethane through the hydrochloric acid, but also suitable for purifying industrial oxammonium hydrochloride products the quality index of which do not reach the reagent level; the industrial oxammonium hydrochloride products are dissolved, filtered and recrystallized according to the conventional recrystallization process to reach the quality standard of the reagent level oxammonium hydrochloride products.
Description
Technical field
The present invention is a kind of method that improves quality of oxammonium hydrochloride.Belong to the preparation of hydroxylamine compound, particularly in the oxammonium hydrochloride preparation process, the method for improving the quality of products.
Background technology
Oxammonium hydrochloride, colourless needle crystal is a kind of important organic synthesis industrial chemicals.Be used for pharmaceutical industry mainly as medicine intermediate, in the prior art, adopt Nitromethane 99Min. and hydrochloric acid hydrolysis method production technique.In hydrolytic process, the by product kind is many, also has the impurity that enters with raw material, is difficult to remove.For example, significantly black oil dissolubility spot, colourless metal pollutant etc.These impurity are difficult to remove clean before the packing of product; In addition, product is between the shelf lives, because product flavescence phenomenon in various degree can appear in the existence of impurity.As the raw material of medicine intermediate product, the client is harsh unusually to the requirement of quality of oxammonium hydrochloride, and the oxammonium hydrochloride Industrial products that adopt prior art processes to produce are difficult to reach the quality standard of pharmaceutical grade oxammonium hydrochloride.
A kind of reduced investment, operating procedure be simple, remove black splotch in the product, make the method that significantly improves quality of oxammonium hydrochloride that product can flavescence between the shelf lives is that people expect.
Summary of the invention
The objective of the invention is to avoid above-mentioned weak point of the prior art, and provide a kind of reduced investment, operating procedure simple, remove black splotch in the product, make the method that significantly improves quality of oxammonium hydrochloride that product can flavescence between the shelf lives.
Purpose of the present invention can reach by following measure:
The method of raising quality of oxammonium hydrochloride of the present invention is characterized in that increasing a filtration unit at least in traditional oxammonium hydrochloride technological process of production, make Nitromethane 99Min. after the hcl acidifying hydrolysis, the oxammonium hydrochloride solution that generates after the filtration unit filtration, enters concentration section again.
Purpose of the present invention can also reach by following measure:
Raising crystal oxammonium hydrochloride method for quality of the present invention is characterized in that adopting vacuum filtration technology, and vacuum degree control is preferred scheme between-0.05Mpa-0.1Mpa.
Raising crystal oxammonium hydrochloride method for quality of the present invention, it is better to it is characterized in that described filtration temperature is controlled at 80 ℃ of-120 ℃ of effects.
The method of raising crystal oxammonium hydrochloride purity of the present invention is characterized in that described filtration unit adopts the corrosion resistant material of stable performance to make.The described preferred scheme of stable corrosion resistant material is any one that chooses from polypropylene, tetrafluoroethylene, pottery, enamel.
Raising crystal oxammonium hydrochloride method for quality of the present invention is characterized in that the filtering accuracy of described filtration unit is chosen between the 0.07-0.2mm, can obtain better effect.
The method of raising quality of oxammonium hydrochloride of the present invention, it is characterized in that not being only applicable to the hydrolysis of Nitromethane 99Min. hcl acidifying and prepare the oxammonium hydrochloride process modification, be applicable to that also quality index does not reach the purification of the technical hydrochloric acid azanol product of SILVER REAGENT as yet, according to traditional recrystallizing technology, after its dissolving, filtration, recrystallization make it reach reagent grade hydrochloric acid azanol target level of product quality easily.
Technical scheme of the present invention has following outstanding substantive distinguishing features compared to existing technology and advances significantly, has produced following positively effect:
1. provide a kind of reduced investment, operating procedure simple, remove black splotch in the product, make the method that significantly improves quality of oxammonium hydrochloride that product can flavescence between the shelf lives;
2. be not only applicable to the hydrolysis of Nitromethane 99Min. hcl acidifying and prepare the oxammonium hydrochloride process modification, be applicable to that also quality index does not reach the purification of the technical hydrochloric acid azanol product of SILVER REAGENT as yet, according to traditional recrystallizing technology, after its dissolving, filtration, recrystallization make it reach reagent grade hydrochloric acid azanol target level of product quality easily;
3. quality product has satisfied the demand of pharmaceutical industry, has improved the economic benefit of oxammonium hydrochloride manufacturing enterprise.
4. product does not have black splotch impurity, store 2 years in nondiscoloration.
Embodiment
The present invention will now be further detailed embodiment:
Embodiment 1
Adopt polypropylene material to make strainer, filtration area 4M
2Terylene filter cloth with filtering accuracy 0.074mm; Control vacuum tightness-0.05Mpa-0.1Mpa, under 80 ℃ of-120 ℃ of conditions of temperature, the oxammonium hydrochloride hydrolyzed solution that hydrolysis is good is by strainer, and the suction concentration tank enters next step technology.
Making product does not have black splotch impurity, store 2 years in nondiscoloration.
Embodiment 2
According to method and the step of embodiment 1, different is to adopt the efficient board-like sealing filter of NYB-4 type, filtering accuracy 0.15mm; Making product does not have black splotch impurity, and product is preserved nondiscoloration in 2 years.
Embodiment 3
According to method and the step of embodiment 1, different is to adopt ZX series self-cleaning type filter element filtering machine, filtration area 4M
2Making product does not have black splotch impurity, and product is preserved nondiscoloration in 2 years.
Embodiment 4
According to method and the step of embodiment 1, select DL series bag type filtering machine for use.Filtering accuracy 0.1mm.; Making product does not have black splotch impurity, and product is preserved nondiscoloration in 2 years.
Embodiment 5
According to method and the step of embodiment 1, select JYF type backpulsing multicore filter for use, filtering accuracy 0.2mm; Making product does not have black splotch impurity, and product is preserved nondiscoloration in 2 years.
Embodiment 6
Commercially available have black splotch impurity, and the oxammonium hydrochloride product of flavescence is dissolved in water with it, filters according to method and the step of embodiment 1, and making product does not have black splotch impurity, store 2 years in nondiscoloration.
Claims (4)
1. a method that improves quality of oxammonium hydrochloride is characterized in that increasing a filtration unit at least in traditional oxammonium hydrochloride technological process of production, make Nitromethane 99Min. after the hcl acidifying hydrolysis, the oxammonium hydrochloride solution that generates after the filtration unit filtration, enters concentration section again.
2. according to the method for the raising quality of oxammonium hydrochloride of claim 1, it is characterized in that adopting vacuum filtration technology, vacuum degree control-0.05Mpa～-0.1Mpa between.
3. according to the method for the raising quality of oxammonium hydrochloride of claim 1, it is characterized in that described filtration temperature is controlled between 80 ℃-120 ℃.
4. according to the method for the raising quality of oxammonium hydrochloride of claim 1, the filtering accuracy that it is characterized in that described filtration unit is between 0.07-0.2mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910018411A CN101659402A (en) | 2009-09-15 | 2009-09-15 | Method for improving quality of oxammonium hydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910018411A CN101659402A (en) | 2009-09-15 | 2009-09-15 | Method for improving quality of oxammonium hydrochloride |
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| Publication Number | Publication Date |
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| CN101659402A true CN101659402A (en) | 2010-03-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN200910018411A Pending CN101659402A (en) | 2009-09-15 | 2009-09-15 | Method for improving quality of oxammonium hydrochloride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236365A (en) * | 2015-09-15 | 2016-01-13 | 山东宝源化工股份有限公司 | Method for producing hydroxylamine hydrochloride by using industrial tail gas absorption waste liquid |
| CN105540559A (en) * | 2016-01-28 | 2016-05-04 | 苏州市吴赣药业有限公司 | Method for improving quality of oxammonium hydrochloride and raising yield of oxammonium hydrochloride |
| CN106946235A (en) * | 2017-03-23 | 2017-07-14 | 北京凯瑞英科技有限公司 | A kind of method that phase-transfer synthesis hydroxylamine hydrochloride is passed through by nitromethane and hydrochloric acid |
| CN108236945A (en) * | 2017-12-22 | 2018-07-03 | 北京凯瑞英科技有限公司 | Heteropoly acid slurry catalyst, preparation and the application in hydroxylamine hydrochloride catalyzes and synthesizes |
-
2009
- 2009-09-15 CN CN200910018411A patent/CN101659402A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236365A (en) * | 2015-09-15 | 2016-01-13 | 山东宝源化工股份有限公司 | Method for producing hydroxylamine hydrochloride by using industrial tail gas absorption waste liquid |
| CN105236365B (en) * | 2015-09-15 | 2017-09-26 | 山东宝源化工股份有限公司 | The method that waste liquid produces hydroxylamine hydrochloride is absorbed using industrial tail gas |
| CN105540559A (en) * | 2016-01-28 | 2016-05-04 | 苏州市吴赣药业有限公司 | Method for improving quality of oxammonium hydrochloride and raising yield of oxammonium hydrochloride |
| CN106946235A (en) * | 2017-03-23 | 2017-07-14 | 北京凯瑞英科技有限公司 | A kind of method that phase-transfer synthesis hydroxylamine hydrochloride is passed through by nitromethane and hydrochloric acid |
| CN106946235B (en) * | 2017-03-23 | 2019-03-22 | 北京凯瑞英科技有限公司 | A method of phase-transfer synthesis hydroxylamine hydrochloride is passed through by nitromethane and hydrochloric acid |
| CN108236945A (en) * | 2017-12-22 | 2018-07-03 | 北京凯瑞英科技有限公司 | Heteropoly acid slurry catalyst, preparation and the application in hydroxylamine hydrochloride catalyzes and synthesizes |
| CN108236945B (en) * | 2017-12-22 | 2021-01-08 | 北京凯瑞英科技有限公司 | Heteropolyacid slurry catalyst, preparation and application in hydroxylamine hydrochloride catalytic synthesis |
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Open date: 20100303 |